CN114031035A - High-energy electron beam in-situ irradiation controllable preparation method of metal nanometer needle point - Google Patents

High-energy electron beam in-situ irradiation controllable preparation method of metal nanometer needle point Download PDF

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CN114031035A
CN114031035A CN202111321921.4A CN202111321921A CN114031035A CN 114031035 A CN114031035 A CN 114031035A CN 202111321921 A CN202111321921 A CN 202111321921A CN 114031035 A CN114031035 A CN 114031035A
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electron beam
irradiation
metal
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nanowire
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苏江滨
潘鹏
季雪梅
何祖明
唐斌
郎咸忠
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Changzhou University
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Abstract

The invention discloses a controllable preparation method of high-energy electron beam in-situ irradiation of a metal nanometer needle point, which is characterized in that an amorphous nanowire with a layer of metal nanometer particles sprayed on the surface is prepared into a Transmission Electron Microscope (TEM) sample, the nanowire is subjected to focused irradiation by using a high-energy electron beam in the TEM, the amorphous nanowire material in an irradiation region is induced to be preferentially melted and steamed and radially shrunk, and meanwhile, the metal nanometer particles on the surface of the nanowire are caused to be linearly aggregated, fused and elongated, and finally, the metal nanometer needle point structure is obtained. The invention utilizes high-energy electron beams in the TEM to not only induce the transformation of the nano structure in a non-thermal activation manner, but also observe the nano processing preparation process in situ with high resolution. In addition, the irradiation processing is only carried out at room temperature, external assistance such as light, heat, electricity, force and the like is not needed, and the whole irradiation preparation process is simple and easy to operate.

Description

High-energy electron beam in-situ irradiation controllable preparation method of metal nanometer needle point
Technical Field
The invention belongs to the technical field of nano material processing, and particularly relates to a high-energy electron beam in-situ controllable preparation method of a metal nano needle tip.
Background
The nano processing technology is an important component for promoting the development of nano technology, and plays an important role in realizing novel micro-nano scale structures and devices such as optics, electronics, semiconductors, sensors and the like. As one of the strongest energy beams, the high-energy electron beam in a transmission electron microscope (transmission electron microscope, TEM for short) can carry out high-resolution in-situ observation on low-dimensional nano materials and can also carry out fine controllable nano processing, thereby showing great superiority. The nano wire is a typical one-dimensional nano material, has large length-diameter ratio, and shows wide application prospect in the fields of micro-nano electronic devices, chemical biosensors and the like. However, conventional cylindrical nanowire structures and associated properties often have difficulty meeting the performance requirements of all types of devices, which requires precise and controlled processing of nanowires on a nanoscale to improve their performance.
With the development of electron microscope technology, the high-energy electron beam in the TEM can realize the change of the shapes of the nanowire such as length, diameter, curvature and the like in situ and the fine nano-processing such as cutting, punching, welding and the like. In addition, the metal nanowire with different thicknesses at two ends and a needle tip shape, namely the metal nanowire tip structure, has attractive application prospect in the technical fields of scanning detection and field emission. In the prior literature, amorphous SiO is achieved by irradiation with high-energy focused electron beamsxSharpening, hooking and welding the nano wires. However, since the stability of the crystalline metal nanowire is higher than that of the amorphous SiOxThe nano-wire is much better, the metal nano-needle tip structure is difficult to prepare by the same method, and the metal nano-needle tip structure is not successfully prepared by high-energy electron beam focusing irradiation in a transmission electron microscope in the prior literature.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above problems occurring in the prior art.
Therefore, the present invention aims at providing a high-energy electron beam in-situ controllable preparation method of a metal nanometer needle tip.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions: a controllable preparation method of high-energy electron beam in-situ irradiation of metal nanometer needle tip comprises,
spraying a layer of metal nano particles on the surface of the amorphous nano wire, dispersing the nano wire on an electron microscope micro-grid to prepare a TEM sample, then loading the TEM sample into a TEM, selecting a nano wire segment with two ends lapped in a micro-grid hole, focusing an electron beam on the radial center of the nano wire segment for continuous irradiation, inducing the amorphous nano wire material in an irradiation area to perform melting evaporation and radial contraction, and simultaneously gradually realizing linear aggregation, fusion and extension of the metal nano particles to finally obtain the metal nano needle tip structure.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the amorphous nanowires include, but are not limited to, amorphous metal nanowires, amorphous semiconductor nanowires, amorphous insulator nanowires, and amorphous composite nanowires.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the diameter of the amorphous nanowire is 20-100nm, the amorphous nanowire is axially straight and has uniform radial thickness, and other impurities are not adsorbed.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the metal nanoparticles include, but are not limited to, various common Au, Ag, Cu, Fe crystalline metal nanoparticles.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the amorphous nanowires are less stable than the metal nanoparticles.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the diameter of the metal nano-particles is 3-8nm, the amorphous nano-wires are arranged in a gradient manner in the radial direction, one side of the amorphous nano-wires is loose, and the other side of the amorphous nano-wires is relatively compact.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the beam spot size of the electron beam is slightly smaller than the diameter of the amorphous nanowire.
As a preferred scheme of the high-energy electron beam in-situ irradiation controllable preparation method of the metal nanometer needle tip, the preparation method comprises the following steps: the acceleration voltage of the electron beam is 200-300 kV; the current density of the irradiation is (0.2-12.5) x 103A/cm2。
The invention has the beneficial effects that:
the invention adopts high-energy electron beams in TEM to carry out in-situ focusing irradiation on the amorphous nanowire modified by the metal nanoparticles, utilizes the structural instability difference of the amorphous nanowire and the crystalline metal nanoparticles, and non-thermally induces the preferential melting evaporation and radial shrinkage of the amorphous nanowire material, and simultaneously causes the metal nanoparticles on the surface of the nanowire to continuously linearly gather, fuse and extend towards the irradiation center, thereby finally obtaining the metal nanometer needle point structure. The invention can effectively control the preparation process of the metal nanometer needle point structure by adjusting the diameter of the amorphous nanometer wire, the type, the size and the distribution of the metal nanometer particles, the beam spot size of the electron beam, the irradiation current density and other parameters.
The high-energy electron beam in-situ irradiation controllable preparation method has the advantages of inducing nano structure transformation through non-thermal activation, simultaneously observing the preparation process of the nano needle tip structure in situ with high resolution and the like. In addition, the irradiation processing is only carried out at room temperature, external assistance such as light, heat, electricity, force and the like is not needed, and the whole irradiation preparation process is simple and easy to operate.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 shows SiO modified by Au nanoparticles selected in example 1xTEM photograph of the nanowire fragment and the position and spot size of the high energy electron beam irradiation (see circle position in the figure);
fig. 2 is a general TEM photograph of the Au nanoprobe tip obtained after the high energy electron beam irradiation of the nanowire segment selected in example 1.
Fig. 3 is a high-resolution TEM photograph of the Au nanoprobe tip obtained after the nanowire segment selected in example 1 is irradiated in situ by the high-energy electron beam, and the inset in the upper right corner is a corresponding Fast Fourier Transform (FFT) image of the tip structure when high resolution is taken.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The embodiment chooses to use amorphous SiOxThe nano-wire, wherein x is 2-3.
Example 1:
(1) TEM sample preparation: using BAL-TEC CoThe produced SCD 005 sputtering coating equipment is used for preparing amorphous SiOxAnd a layer of Au nano particles is deposited on the surface of the nanowire, and the deposition time is 5 s. Then, a little modified SiO is addedxNanowire powder (<<1mg) is ultrasonically dispersed in absolute ethyl alcohol with the mass fraction of more than or equal to 99.7 percent, then a dropper is used for sucking the suspension liquid drop 2 containing the nano wire to be dripped on an electron microscope micro-grid, and a TEM sample is obtained after drying.
(2) Nanowire sample screening: the TEM samples were loaded into a Tecnai F30 field emission TEM for sample screening. As shown in FIG. 1, the diameter of the selected nanowire is 45nm, the nanowire is axially straight and has uniform radial thickness, and both ends of the nanowire are lapped on the micro-grid hole (the edge of the hole cannot be seen in the figure). The surface of the nanowire is modified with a layer of Au nanoparticles which are distributed along the radial gradient and have the size of 3-8nm, and the whole nanowire has a surface appearance that one side of the nanowire is sparse and the other side of the nanowire is relatively dense.
(3) Electron beam irradiation processing: firstly, the beam spot size of the electron beam is adjusted to be 25nm, and the irradiation current density is adjusted to be 2.0 multiplied by 103A/cm2The accelerating voltage is 300kV, then the nanowire is focused on the radial center of the nanowire for in-situ irradiation processing (see figure 1), the nanowire gradually shrinks radially in the irradiation range and finally breaks, and meanwhile, Au nanoparticles on the surface of the nanowire gradually linearly gather, fuse and extend to form an Au nanometer needle point structure (see figure 2). In order to characterize the microstructure of the Au nano-tip, a high-resolution TEM photograph of the Au nano-tip and a corresponding FFT image were further taken, and as shown in fig. 3, the Au nano-tip was determined to be a crystalline structure.
Example 2:
(1) TEM sample preparation: amorphous SiO by using SCD 005 sputtering coating equipment produced by BAL-TEC companyxAnd a layer of different metal nano particles is deposited on the surface of the nano wire, and the deposition time is 5 s. Then, a little modified SiO is addedxNanowire powder (<<1mg) is ultrasonically dispersed in absolute ethyl alcohol with the mass fraction of more than or equal to 99.7 percent, then a dropper is used for sucking the suspension liquid drop 2 containing the nano wire to be dripped on an electron microscope micro-grid, and a TEM sample is obtained after drying.
(2) Nanowire sample screening: the TEM samples were loaded into a Tecnai F30 field emission TEM for sample screening. The diameter of the nanowire selected in this embodiment is 45nm, and a layer of metal nanoparticles distributed in a gradient manner along the radial direction and having a size of 3-8nm is modified on the surface of the nanowire.
(3) Electron beam irradiation processing: firstly, the beam spot size of the electron beam is adjusted to be 25nm, and the irradiation current density is adjusted to be 2.0 multiplied by 103A/cm2The accelerating voltage is 300kV, then the nanowire is focused on the radial center of the nanowire for in-situ irradiation processing, the nanowire gradually shrinks radially in the irradiation range and finally breaks, and meanwhile, the metal nanoparticles on the surface of the nanowire gradually linearly gather, fuse and extend to form a metal nanometer needle tip structure. The structures of the tips of the prepared nanoparticles of different metals are shown in table 1.
TABLE 1 Nanocoip structures prepared from different metal nanoparticles
Figure BDA0003345829680000051
The kind of the metal nanoparticles determines the kind of the nano-needle tip, and as shown in table 1, the metal nanoparticles can be various common crystalline metal nanoparticles such as Au, Ag, Cu, Fe, etc., and the stability of the metal nanoparticles is higher than that of the amorphous nanowires. Therefore, the amorphous nanowire material can be continuously melted and steamed by the electron beam, and simultaneously the relative stability of the metal nanoparticles can be ensured, and the metal nanoparticles are gathered together through diffusion and migration to be fused into a linear structure.
Example 3:
(1) TEM sample preparation: amorphous SiO by using SCD 005 sputtering coating equipment produced by BAL-TEC companyxAnd a layer of Au nano particles is deposited on the surface of the nanowire, and the deposition time is 5 s. Then, a little modified SiO is addedxNanowire powder (<<1mg) is ultrasonically dispersed in absolute ethyl alcohol with the mass fraction of more than or equal to 99.7 percent, then a dropper is used for sucking the suspension liquid drop 2 containing the nano wire to be dripped on an electron microscope micro-grid, and a TEM sample is obtained after drying.
(2) Nanowire sample screening: the TEM samples were loaded into a Tecnai F30 field emission TEM for sample screening. The diameters of the nanowires selected in the embodiment are 45nm and 60nm respectively, and a layer of Au nanoparticles which are distributed in a gradient manner or uniformly in the radial direction and have the size of 3-8nm is modified on the surface of the nanowire.
(3) Electron beam irradiation processing: the size of the beam spot of the electron beam and the corresponding irradiation current density are adjusted as shown in table 2, the accelerating voltage is 300kV, then the electron beam is focused on the radial center of the nanowire for in-situ irradiation processing, the nanowire gradually shrinks radially in the irradiation range and finally breaks, and meanwhile, Au nanoparticles on the surface of the nanowire are gradually linearly gathered, fused and elongated to form an Au nano needle point structure.
TABLE 2 Effect of different electron beam spot sizes on the Metal NanoTab Structure
Figure BDA0003345829680000052
Figure BDA0003345829680000061
As shown in table 2, the beam spot size of the electron beam is required to be slightly smaller than the diameter of the amorphous nanowire. If the beam spot size is too small, perforation of the nanowires is likely to occur. The reason is that the electron beam spot is too small, the irradiation current density is large, the electron beam induces the amorphous nanowire material in the small irradiation area to carry out rapid melting and evaporation, and the peripheral unirradiated area can still keep the structural stability without collapse due to the passivation effect of the metal nanoparticles, so that the hole structure is obtained. On the contrary, if the size of the beam spot of the electron beam is slightly larger than the diameter of the nanowire and the particles are uniformly distributed, a dumbbell-shaped structure rather than a needle point structure is easily obtained. The reason is that when the size of the beam spot is slightly larger than the diameter of the nanowire and is focused on the center of the nanowire, the irradiation effect at the center of the beam spot is stronger than that at the edge, symmetric necking appears at two sides of the nanowire, the center shrinks fast, the edge shrinks slowly, and simultaneously metal particles uniformly distributed at two sides are continuously gathered towards the central axis of the nanowire, close to each other and grow in a fusion manner, so that a dumbbell-shaped structure is finally formed.
Example 4:
(1) TEM sample preparation: amorphous SiO by using SCD 005 sputtering coating equipment produced by BAL-TEC companyxDepositing a layer of Au nano on the surface of the nano wireParticles, deposition time 5 s. Then, a little modified SiO is addedxNanowire powder (<<1mg) is ultrasonically dispersed in absolute ethyl alcohol with the mass fraction of more than or equal to 99.7 percent, then a dropper is used for sucking the suspension liquid drop 2 containing the nano wire to be dripped on an electron microscope micro-grid, and a TEM sample is obtained after drying.
(2) Nanowire sample screening: the TEM samples were loaded into a Tecnai F30 field emission TEM for sample screening. The diameter of the selected nanowires in this example is shown in table 3, and the nanowires are axially straight and uniform in radial thickness. The surface of the nanowire is modified with a layer of Au nanoparticles which are distributed along the radial direction in a gradient manner and have the size of 3-8 nm.
(3) Electron beam irradiation processing: the electron beam spot size and the corresponding irradiation current density are adjusted according to the diameter of the nanowire, as shown in table 3, the acceleration voltage is 300kV, then the nanowire is focused on the radial center of the nanowire for in-situ irradiation processing, the nanowire gradually shrinks radially in the irradiation range and finally breaks, and meanwhile, Au nanoparticles on the surface of the nanowire gradually and linearly gather, fuse and extend to form an Au nano needle point structure.
TABLE 3 different amorphous SiOxEffect of nanowire diameter on Metal NanoTab Structure
Figure BDA0003345829680000062
Figure BDA0003345829680000071
As can be seen from Table 3, for amorphous SiOxFor nanowires, the ideal diameter is between 20-100nm, and it is not appropriate that the nanowires are too thick or too thin. When the nano-wire is too thin, namely below 20nm, the metal nano-particles are not easy to be arranged in a gradient manner, and the amorphous nano-wire material cannot be stably sequenced in the process of being continuously melted and steamed by the electron beam, so that a proper nano-needle tip structure cannot be prepared. While too thick a nanowire exceeds the linearity requirements of the nanostructure (0.1-100nm) and is not studied or discussed here.
The type of the metal nano-particles determines the type of the nano-needle tips, and the metal nano-particles can be various common crystalline metal nano-particles such as Au, Ag, Cu, Fe and the like, and the stability of the metal nano-particles is higher than that of amorphous nano-wires. Therefore, the amorphous nanowire material can be continuously melted and steamed by the electron beam, and simultaneously the relative stability of the metal nanoparticles can be ensured, and the metal nanoparticles are gathered together through diffusion and migration to be fused into a linear structure. The size of the metal nanoparticles affects their diffusion, migration and fusion processes closely related to surface energy, with particles of 3-8nm diameter being preferred. Moreover, the distribution of the metal nano particles on the surface of the amorphous nano wire requires that the metal nano particles are arranged in a certain gradient along the radial direction of the nano wire, one side of the metal nano particles is sparse, and the other side of the metal nano particles is relatively dense. Thus facilitating the directional diffusion and migration of the particles from the sparse side to the dense side, and finally arranging the particles in a linear structure on the dense side. With the continuous irradiation, the amorphous nanowires will accelerate radial shrinkage and fracture, and in the process, the nanowires will generate stretching action along the axial direction, so that the metal linear structure softened under the irradiation of the high-energy electron beams will be elongated into a nanometer needle point structure.
The beam spot size of the electron beam is required to be slightly smaller than the diameter of the amorphous nanowire. If the size of the beam spot of the electron beam is slightly larger than the diameter of the nanowire and the particles are uniformly distributed, a dumbbell-shaped structure rather than a needle point structure is easily obtained. In addition, the acceleration voltage of the electron beam is 200-300kV, and the irradiation current density is (0.2-12.5) × 103A/cm2. Under the condition, the melting evaporation and radial shrinkage of the amorphous nanowire material, the aggregation, fusion, elongation and other structural transformations of the metal nanoparticles can be ensured.
In conclusion, the preparation process and the final appearance of the metal nanometer needle point structure can be controlled by adjusting the diameter of the amorphous nanometer wire, the type, the size and the distribution of the metal nanometer particles modified on the surface, the beam spot size of the electron beam, the accelerating voltage, the irradiation current density and other parameters.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (8)

1. A high-energy electron beam in-situ irradiation controllable preparation method of a metal nanometer needle point is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
spraying a layer of metal nano particles on the surface of the amorphous nano wire, dispersing the nano wire on an electron microscope micro-grid to prepare a TEM sample, then loading the TEM sample into a TEM, selecting a nano wire segment with two ends lapped in a micro-grid hole, focusing an electron beam on the radial center of the nano wire segment for continuous irradiation, inducing the amorphous nano wire material in an irradiation area to perform melting evaporation and radial contraction, and simultaneously gradually realizing linear aggregation, fusion and extension of the metal nano particles to finally obtain the metal nano needle tip structure.
2. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the amorphous nanowires include, but are not limited to, amorphous metal nanowires, amorphous semiconductor nanowires, amorphous insulator nanowires, and amorphous composite nanowires.
3. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the diameter of the amorphous nanowire is 20-100nm, the amorphous nanowire is axially straight and has uniform radial thickness, and other impurities are not adsorbed.
4. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the metal nanoparticles include, but are not limited to, various common Au, Ag, Cu, Fe crystalline metal nanoparticles.
5. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the amorphous nanowires are less stable than the metal nanoparticles.
6. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the diameter of the metal nano particles is 3-8nm, the metal nano particles are arranged in a gradient manner in the radial direction of the amorphous nanowire, one side of the metal nano particles is loose, and the other side of the metal nano particles is relatively compact.
7. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the beam spot size of the electron beam is slightly smaller than the diameter of the amorphous nanowire.
8. The controllable preparation method of high-energy electron beam in-situ irradiation of the metal nanometer needle tip as claimed in claim 1, characterized in that: the acceleration voltage of the electron beam is 200-300 kV; the current density of the irradiation is (0.2-12.5) x 103A/cm2。
CN202111321921.4A 2021-11-09 2021-11-09 High-energy electron beam in-situ irradiation controllable preparation method of metal nanometer needle point Pending CN114031035A (en)

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